1、Designation: D 7066 04An American National StandardStandard Test Method fordimer/trimer of chlorotrifluoroethylene (S-316) RecoverableOil and Grease and Nonpolar Material by InfraredDetermination1This standard is issued under the fixed designation D 7066; the number immediately following the designa
2、tion indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the dete
3、rmination of oil andgrease and nonpolar material in water and wastewater by aninfrared (IR) determination of dimer/trimer of chlorotrifluoro-ethylene (S-316) extractable substances from an acidifiedsample. Included in this estimation of oil and grease are anyother compounds soluble in the solvent.1.
4、2 The method is applicable to measurement of the lightfuel although loss of some light ends during extraction can beexpected.1.3 This method defines oil and grease in water and waste-water as that which is extractable in the test method andmeasured by IR absorption at 2930 cm-1or 3.4 microns.Similar
5、ly, this test method defines nonpolar material in waterand wastewater as that oil and grease which is not adsorbed bysilica gel in the test method and measured by IR absorption at2930 cm-1.1.4 This method covers the range of 5 to 100 mg/L and maybe extended to a lower or higher level by extraction o
6、f a largeror smaller sample volume collected separately.1.5 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine (D 3856Guide for
7、Good Laboratory Practices2) the applicability ofregulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 3370 Practices for Sampling Water from Closed ConduitsD 3856 Guide for Good Laboratory Practices E
8、ngaged inSampling and Analysis of WaterD 2777 Practice for the Determination of Precision andBias of Applicable Methods of Committee D19 on WaterD 5810 Guide for Spiking into Aqueous SamplesD 5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE 168 Pr
9、actices for General Techniques of Infrared Quanti-tative AnalysisE 178 Practice for Dealing With Outlying Observations3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D 1129 and Practices E 168.3.2 Definitions of Terms Specific to This Standard:3.2.
10、1 oil and greasethe organic matter extracted fromwater or wastewater and measured by this test method.3.2.2 nonpolar materialthe oil and grease remaining insolution after contact with silica gel and measured by this testmethod.3.2.3 solventdimer/trimer of chlorotrifluoroethylene (S-316)4. Summary of
11、 Test Method4.1 An acidified 250-mL sample of water or wastewater isextracted serially with three 15-mL volumes of dimer/trimer ofchlorotrifluoroethylene (S-316). The extract is diluted to 50mLand a portion is examined by infrared spectroscopy (IR) for anoil and grease measurement.3A portion of the
12、extract iscontacted with silica gel to remove polar substances, therebyproducing a solution containing nonpolar material. The non-polar material is measured by infrared spectroscopy.5. Significance and Use5.1 The presence and concentration of oil and grease indomestic and industrial wastewater is of
13、 concern to the publicbecause of its deleterious aesthetic effect and its impact onaquatic life.5.2 Regulations and standards have been established thatrequire monitoring of oil and grease in water and wastewater.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the di
14、rect responsibility of Subcommittee 19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved June 1, 2004. Published July 2004.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of AST
15、MStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Consult the manufacturers operation manual for the specific instructionsrelated to the infrared spectrometer or analyzer to be used.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
16、Conshohocken, PA 19428-2959, United States.6. Interferences6.1 Soaps, detergents, surfactants and other materials mayform emulsions that may reduce the amount of oil and greaseextracted from a sample. This test method contains proceduresthat can assist the analyst in breaking such emulsions.6.2 Orga
17、nic compounds and other materials not consideredas oil and grease on the basis of chemical structure may beextracted and measured as oil and grease. Of those measured,certain ones may be adsorbed by silica gel while others maynot. Those not adsorbed are measured as nonpolar material.7. ApparatusAll
18、glassware that will come in contact with the sample mustbe rinsed with dimer/trimer of chlorotrifluoroethylene (S-316)prior to beginning this procedure.7.1 Cell(s), quartz, 10-mm path length (lower concentra-tions may require a longer pathlength), two required fordouble-beam operation, one required
19、for single-beam opera-tion, or built-in or drop-in cell for infrared filtometer analyzeroperation.7.2 Filter Paper, ashless, quantitative, general-purpose, 11-cm, Whatman #40 or equivalent.7.3 Glass Funnel7.4 Glass Wide Mouth Sample Bottle, minimum 250-mL,with screw cap having a fluoropolymer liner.
20、7.5 Glass Graduated Cylinder, 100-mL7.6 Infrared Spectrometer, double-beam dispersive, single-beam dispersive, Fourier transform, filtometers or other ca-pable of making measurements at 2930 cm-1.7.7 Magnetic Stirrer, with small TFE-fluorocarbon stirringbar.7.8 Glass Separatory-Funnel, 500mL, with f
21、luoropolymerstopcock and stopper.7.9 Volumetric Flasks, glass, various (10, 25, 50, 100, and200-mL)7.10 Teflon spritz bottle, one-piece wash bottle for rinsing7.11 Repeating pipetter, glass, 15-mL, (optional)7.12 Volumetric Pipettes, glass, various (0.50, 1.00, 5.00,10.0 and 25.0-mL, including a 1.0
22、0 serological pipet graduatedin 0.01-mL increments and a 5.00-mL serological pipet gradu-ated in 0.1-mL increments, or equivalent)7.13 Benchtop shaker, (optional)7.14 Glass Stirring Rod, (optional)7.15 Analytical Balance,7.16 Syringes, 50 and 500 mL8. Reagents8.1 Purity of ReagentsReagent grade chem
23、icals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specification of the Committeeon Analytical Reagents of the American Chemical Society,where such specifications are available. Other grades may beused, provided it is first ascertained t
24、hat the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, referencesto laboratory or reagent water shall be understood to meanreagent water conforming to Specification D 1193, Type II.8.3 Isooctan
25、e (2,2,4-trimethylpentane) 98 % minimum pu-rity, for use in calibration.8.4 Octanoic acid 98 % minimum purity, for use in calibra-tion.8.5 Silica Gel, Anhydrous, 75 - 150 micrometers, DavisilGrade 923 (Supelco 21447-7A, or equivalent). Dry at200250C for 24 hour minimum and store in a desiccator orti
26、ghtly sealed container. Determine the dimer/trimer of chlo-rotrifluoroethylene (S-316) soluble material content of thesilica gel by extracting 10 g of silica gel with 25 mL ofdimer/trimer of chlorotrifluoroethylene (S-316) and collect theelute in a flask. Filter and fill a quartz cell for analysis b
27、y IR.The dimer/trimer of chlorotrifluoroethylene (S-316) solublematerial must be less than 5 mg/L.8.6 Sodium Sulfate (Na2SO4), ACS, granular anhydrous.Dry at 200-250 C for 24 hours minimum and store in a tightlysealed container until use. (Note: Powdered sodium sulfateshould not be used because wate
28、r may cause it to solidify.)8.7 Solvent - dimer/trimer of chlorotrifluoroethylene,IRspectroscopy grade, for example S-316 manufactured byHoriba Instruments, Irvine CA, 800-446-7422 (ASTM does notadvocate the use of one vendor over another)8.8 Sulfuric Acid (1 + 1)Slowly and carefully add 1volume of
29、sulfuric acid (H2SO4, sp gr 1.84) to 1 volume ofwater, stirring and cooling the solution during the addition(optional HCl replacement).8.9 Hydrochloric acid, ACS, 1 + 1. Mix equal volumes ofconcentrated HCl and water8.10 Sodium Chloride (NaCl), crystalline, ACSor use inbreaking emulsions, if needed.
30、 Wet thoroughly with solventbefore using.9. Sampling9.1 Collect the sample in accordance with the principlesdescribed in Practices D 3370, using a glass bottle equippedwith a screw cap having a fluoropolymer liner. Prerinse thesample bottle and cap with the solvent prior to samplecollection. Do not
31、rinse the sample bottle with the sample to beanalyzed. Fill bottle with minimal headspace to prevent loss ofvolatile constituants. Do not allow the sample to overflow thebottle during collection. Preventing overflow may not bepossible in all sampling situations, however, measures shouldbe taken to m
32、inimize overflow at all times.9.2 A sample of about 250mL is required for this test. Usethe entire sample because removing a portion would notapportion the oil and grease that adheres to the bottle surfaces.The high probability that extractable matter may adhere tosampling equipment and result in me
33、asurements that are biasedlow precludes the collection of composite samples for deter-mination of oil and grease. Therefore, samples must becollected as grab samples. If a composite measurement isrequired, individual grab samples collected at prescribed timeintervals may be analyzed separately and t
34、he concentrationsaveraged. Alternatively, samples can be collected in the fieldand composited in the laboratory. For example, collect fourindividual 63-mL samples over the course of a day. In thelaboratory, pour each 63-mL sample into the separatory funnel,rinse each of the four bottles (and caps) s
35、equentially with10mLof solvent, and use the solvent for the extraction (SectionD706604212.2.2). Do not exceed 50 mL of total solvent during theextraction and rinse procedure.9.3 Preserve the sample with a sufficient quantity of eithersulfuric (see Section 8.8) or hydrochloric acid (see Section 8.9)t
36、o a pH of 2 or lower and refrigerate at 0-4 C from the timeof collection until extraction. The amount of acid required willbe dependent upon the pH and buffer capacity of the sample atthe time of collection. If the amount of acid required is notknown, make the pH measurement on a separate sample tha
37、twill not be analyzed. Introduction of pH paper to an actualsample or sample cap may remove some oil from the sample.To more accurately calculate the final oil concentration of theextract, the volume of acid added to each sample can berecorded, then subtracted from the final measured samplevolume.If
38、 the sample is to be shipped by commercial carrier, U.S.Department of Transportation regulations limit the pH to aminimum (see 40CFR Part 136, Table II Footnote 3) of 1.96 ifHCl is used and 1.15 if H2SO4is used (see 49 CFR part 172).Collect an additional 1 or 2 sample aliquots for the matrix spikean
39、d matrix spike duplicate (Section 14.5) and preserve withacid.9.4 Refrigerate the sample at 15 %, a calibration curve must be used or the calibrationstandards must be adjusted to bound the linear range (seeSection 11 note). Either the average calibration factor (CFm)orthe calibration curve is used,
40、not both. Verification is done onthe chosen calibration.11.12 Verify calibration after each 10 analyses using cali-bration solution C or D, or alternating the calibration solutions.Calibration is verified if CFXis within +/- 15 % of CFmor itsrespective point on the calibration curve.11.13 If calibra
41、tion is not verified, prepare a fresh calibra-tion solution and repeat the calibration verification test (Section11.12). If calibration is not verified with the fresh calibrationstandard, recalibrate and reanalyze all extracts of all samplesanalyzed since the last calibration or verification, whiche
42、ver ismost recent.12. Procedure12.1 Sample pretreatment12.1.1 Bring the sample and QC (i.e., MS/MSD) aliquots toroom temperature.12.1.2 Either mark the sample bottle at the water meniscusor weigh the bottle for later determination of the samplevolume. Weighing will be more accurate.12.2 Extraction:1
43、2.2.1 Transfer the sample from the sample bottle to a cleanseparatory funnel via a clean transfer funnel.12.2.2 Place a filter paper in a filter funnel, add approxi-mately1gofNa2SO4, rinse with a small portion of solvent anddiscard the rinsate.NOTE 5Use of the sodium sulfate is necessary to prevent
44、water frominterfering in the determination. Because the sample is extracted threetimes, it is not necessary to remove all of the solvent from the separatoryD7066044funnel; it is better to preclude water from reaching the sodium sulfate. Ifthe sodium sulfate cakes when contacted with the extract, flu
45、sh once with2 mL of solvent into the 50-mL volumetric flask. Remove the solid witha clean spatula, and add about1goffresh sodium sulfate to the filter.Rewet sodium sulfate with solvent before use.12.2.3 Add 15 mL of solvent to the sample bottle. Cap withthe original cap and shake the sample bottle t
46、o rinse all interiorsurfaces. Pour the solvent into the separatory funnel, rinsingdown the sides of the transfer funnel.12.2.4 Extract the sample by shaking the separatory funnelvigorously for 2 minutes with periodic venting into a hood torelease excess pressure. Vent the funnel slowly to prevent lo
47、ssof sample.12.2.5 Allow the phases to separate.12.2.6 Drain the solvent (lower) layer from the separatoryfunnel through the sodium sulfate into a pre-cleaned 50-mLvolumetric flask.NOTE 6Certain types of samples, such as those containing a largeamount of detergent, may form an emulsion during the ex
48、traction. Ifemulsion forms between the phases and the emulsion is greater thanone-third the volume of the solvent layer, the laboratory should employemulsion-breaking techniques to complete the phase separation. Theoptimum technique depends upon the sample, but may include stirring,filtration throug
49、h glass wool, use of solvent phase separation paper,centrifugation, use of an ultrasonic bath with ice, addition of NaCl,increasing the temperature, lowering the pH, or other physical methods.Alternatively, solid-phase extraction (SPE), continuous liquid-liquid ex-traction, or other extraction techniques may be used to prevent emulsionformation. If such an emulsion cannot be broken by any attempted means,the test method is not applicable to the problem sample. Do not attempt toproceed since accurate, quantitative results for the test are not obtainable.12.2.7 Repeat the
